CN102432747B - Amine lactone type amphoteric high polymer emulsion as well as preparation method and application thereof - Google Patents
Amine lactone type amphoteric high polymer emulsion as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an amine lactone type amphoteric high polymer emulsion as well as a preparation method and application thereof. The amine lactone type amphoteric high polymer emulsion is characterized in that a sulfobetaine type amphoteric ionic monomer and more than one acrylamide nonionic monomer are copolymerized by adopting an inverse emulsion polymerizing method to obtain a high polymer with nonionic copolymer characteristic and salt tackifying effect. Preferably, white oil is used as a dispersion phase, and the HLB (Hydrophile-Lipophile Balance) value of an emulsifying agent is 4.5-5.5. The amine lactone type amphoteric high polymer emulsion prepared by adopting an emulsion polymerization mode has the advantages of high solid content, high dissolvability and relative uniformity in relative molecular mass distribution. The polymer emulsion is easy to disperse and dissolve in fresh water and high-salinity saline water and is very convenient to apply.
Description
Technical field
The present invention relates to a kind of emulsion polymer that is applied to oilfield exploitation, particularly relate to a kind of amine lactone type amphoteric macromolecule polymer emulsion with salt solution tackify character and its production and use.
Background technology
Amphiphatic high polymer is the polymkeric substance that simultaneously contains positive and negative charge group on molecular chain, also referred to as polyamphoteric electrolyte, because it has unique solution effect, can be applicable to multiple fields such as industrial novel material and additive, as oilfield exploitation, water treatment, water-absorbing material, medicine etc.
Amphiphatic high polymer is roughly divided into two classes: a class be acid and alkaline group on same chain link, be called polymer amine lactone (polymeric betains); Another kind of acid and alkaline group, on different chain links, according to the character of monomeric unit, can be divided into strong acid and strong base type, strong acid weak base type, weak acid strong base, weak acid and weak base type.The electric neutrality polymkeric substance that wherein on amine lactone type polymer and macromolecular chain, positive and negative charge group number is equal has anti-polyelectrolyte solution behavior.In the aqueous solution, the electrostatic attraction in molecular chain make in molecular radical and molecular chain in be easy to produce association, cause that its molecular chain shrinks, hydromeehanics size reduces, molecular configurations is comparatively tight; And in salts solution, owing to associating by small molecule salt shielding in molecular radical and in molecular chain, destroying, the enhancing of polymer-solvent phase mutual effect ability, molecular configurations are unfolded more, show obvious anti-polyelectrolyte effect.
At present, amphoteric ion polymer existing institute in three displacement of reservoir oils reports, main method be by AM with just, negative ion monomer carries out radical copolymerization and obtains, as acrylamide/2-acrylamide-2-methylpro panesulfonic acid/acrylamido oxypropyl trimethyl ammonium chloride (AM/AMPS/APDAC) multipolymer, acrylamide/2-acrylamide-2-methylpro panesulfonic acid/MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (AM/AMPS/DMC) multipolymer, the temperature resistant antisalt treatment agent CPS-2000 that also has drilling fluid to use, viscosity-depression agent XY27 and coating agent FA-367, FT-213 etc. for oil recovery profile control, these mostly are the amphoteric ion polymer of the amphoteric ion polymer of cation chain link and negatively charged ion chain link, its aqueous solution has shown certain anti-salt effect, along with the increase of NaCl strength of solution, though its viscosity declines but has higher conservation rate, can reach more than 93%.But in this type of amphoteric ion copolymer, negative ions monomer is on different chain links, ratio regulates difficulty to be difficult to, be difficult to obtain complete electroneutral amphoteric ion copolymer, whole molecular chain can show positive polarity or electronegativity, and its electrostatic interaction both can be repulsive force, also can be magnetism, in strong acid or strong base solution, on superpolymer, there are a large amount of net charges, molecular chain expansion, its behavior is similar to positively charged ion or anionic polyelectrolyte, and the molecular chain of polyamphoteric electrolyte shrinks when iso-electric point.
The synthetic method of Amphiphatic high polymer has: the polymerization of different zwitterion monomers, zwitter-ion to copolymerization monomer polymerization, betaine type amphoteric monomer polymerization, polymerization after the method such as reaction kinetic or macromole reaction of pendant group.The reaction conditionss such as proportioning raw materials must be strictly controlled in the polymerization of different zwitterion monomers just can obtain on molecular chain the equal or approximately equalised amphiphilic polymers of positive and negative charge group number; There is the zwitter-ion of polymerization activity to being normally prepared from by vinyl cationic monomer and the vinyl anionic monomer of identical mole number under certain condition, require can not contain inorganic ion (Na in copolymerization system
+, Cl
-) ion of non-polymeric reactive behavior of class, if 4-vinylpridine/p styrene sulfonic acid salt ion is to comonomer; Betaine type amphoteric monomer is to apply so far many class function monomers, conventionally have carboxylic acid betaine type and sulphonic acid betaine type, wherein sulphonic acid betaine type ampholytic monomer chemistry and Heat stability is good, hydratability strong and contain be not subject to that pH value affects etc. number quaternary ammonium cation and sulfonate anionic.
In sum, in prior art, conventional amphoteric ion polymer mostly is the amphoteric ion polymer of cation chain link and negatively charged ion chain link, and its viscosity is subject to the impact of salinity larger; Do not show electrical amphoteric ion polymer and there is Antipolyelectrolyte property, polymer molecule entirety, the salt resistance having had, but the pure amphoteric ion polymer of reporting in existing document, if poly (AM-co-DMPS) (is acrylamide and methylacryoyloxyethyl-N, the multipolymer of N '-dimethyl-N-propanesulfonic acid amine salt), molecular weight is not high, can not serve as salt-resistant polymer oil displacement agents and improve recovery ratio for offshore oilfield.
Summary of the invention
Object of the present invention is just to provide that a kind of molecular weight is adjustable, soluble in water, the amine lactone type Amphiphatic high polymer with anti-polyelectrolyte solution behavior and preparation method and the purposes of inverse emulsion polymerization thereof.In this high-polymer molecular chain acid, base groups on same chain link and positive and negative electric charge equate, in water, general performance goes out the characteristic of non-ionic copolymer, has the characteristic of salt tackify.Adopt the preparation method of inverse emulsion polymerization, reaction process easily controls, simple to operate, can obtain the amine lactone type amphoteric macromolecule polymer emulsion of higher molecular weight, and this polymer emulsion is soluble in water, in can being applied to easily drilling well and recovering the oil.
One of the present invention's amine lactone type amphoteric macromolecule polymer emulsion, it is characterized in that described emulsion comprises the polymkeric substance being obtained by the sulphonic acid betaine type Amphiphatic high polymer monomer of following general formula: (illustrate: the compound with following structure can be called sulphonic acid betaine type, and what industrial application was more is the sulphonic acid betaine type tensio-active agent that does not contain polymerisable ethylene linkage in its R group)
The wherein integer of n=2～4;
Wherein R is selected from one of lower array structure:
CH
2＝CH-COOCH
2CH
2-，CH
2＝CH-CONHCH
2CH
2-
Described amine lactone type amphoteric macromolecule polymer emulsion is to prepare as raw material adopts inverse emulsion polymerization taking the component of following weight percent, wherein,
Non-ionic acrylamide monomers 10～35%;
Sulphonic acid betaine type zwitterionic monomer 3～20%;
Oil phase 10～30%;
Initiator 0.1～0.8%;
Emulsifying agent 3～10%;
Molecular weight regulator 0.01～0.5%;
Water surplus.
In concrete enforcement,
Described non-ionic acrylamide monomers is selected from acrylamide, N hydroxymethyl acrylamide, N,N-DMAA, N-ethyl acrylamide, N, the combination of one or more in N-diethyl acrylamide, N-propyl group acrylamide;
Described oil phase is selected from alkane, diesel oil, aviation kerosene, white oil; Preferably 5～26# white oil;
Described initiator is made up of Oxidizing and Reducing Agents, and oxygenant is wherein selected from the one in Potassium Persulphate, ammonium persulphate, hydrogen peroxide, and reductive agent is selected from the one in sodium bisulfite, Tetramethyl Ethylene Diamine;
Described molecular weight regulator is the compound that contains sulfydryl;
Described emulsifying agent is non-ionic type compound emulsifying agent, and described non-ionic type compound emulsifying agent carries out composite making by spans tensio-active agent and Tweens tensio-active agent or polyethenoxy ether class tensio-active agent; Comparative optimization, described spans tensio-active agent is selected from least one in Span-85, Span-80, Span-60; Described Tweens tensio-active agent is selected from least one in Tween-80, Tween-60; Described polyethenoxy ether class tensio-active agent is OP-10;
HLB (the being hydrophile-lipophile balance value) value of described non-ionic type compound emulsifying agent is 4～7, preferably 4.5～5.5.
The preparation method of the present invention's two amine lactone type amphoteric macromolecule polymer emulsion comprises the steps:
(1) prepare water: by water miscible zwitterionic monomer and acrylamide monomers, and molecular weight regulator is dissolved in deionized water, logical nitrogen deoxygenation, adds complexing agent, and described complexing agent is disodium edta.
(2) prepare oil phase: composite emulsifying agent is dissolved in to white oil, fully stirs, emulsifying agent is fully dissolved, form uniform oil-phase solution;
(3) emulsification: under high-speed stirring, water is slowly splashed in oil phase, logical nitrogen deoxygenation 20～30 minutes, forms uniform tiny emulsion;
(4) polyreaction: drip the aqueous solution of reductive agent and the aqueous solution of oxygenant in the good W/O of above-mentioned emulsification (water-in-oil) emulsion, keeping temperature is 20～60 DEG C, continue reaction 1～4 hour, obtain the amine lactone type emulsion polymerization of oyster white homogeneous thickness.
Adopt the preparation method of inverse emulsion polymerization, reaction process easily controls, simple to operate, and the solid content of polymer emulsion is between 20～40%, and the intrinsic viscosity of Amphiphatic high polymer can be controlled between 3～15dL/g.
The present invention's three is amine lactone type amphoteric macromolecule polymer emulsion purposes as oil-displacing agent in oilfield exploitation, water treatment, water-absorbing material, medicine, the purposes of the anti-salt oil-displacing agent that particularly drilling fluid tackifier and agent for improving oilfield recovery are used under high salinity.
In the present invention, synthetic amine lactone type amphoteric macromolecule polymer emulsion is exactly to utilize acid, sulphonic acid betaine type zwitterionic monomer and the neutral monomer copolymerization of base groups on same chain link to form, the static charge of the amphiphilic polymers obtaining in the aqueous solution is always zero, has obvious anti-polyelectrolyte effect.There is the sulphonic acid betaine type zwitterionic monomer of bibliographical information to have vinylpyridine piperidine derivatives (as drone salt (4-VPPS) in 4-vinyl-1-(3-sulfopropyl) pyridine) (polymer journal 2009 (4)), acrylamide derivative (as acrylamide ethyl-N, N '-dimethyl-N-propanesulfonic acid amine salt), methacrylate derivative (as methylacryoyloxyethyl-N, N '-dimethyl-N-propanesulfonic acid amine salt (DMPS)).Wherein methylacryoyloxyethyl-N, N '-dimethyl-N-propanesulfonic acid amine salt (DMPS) has report (as J.Mater.Chem.1997,7 (9), petrochemical complex 2006 (3), CN1772778 etc.) in many sections of documents.The zwitterionic monomer that contains " N; N '-dimethyl " on quaternary ammonium salt group also has N, N '-dimethyl-N-(2-methylacryoyloxyethyl)-N-(3-propyl sulfonic acid ammonium inner salt) is (US3497482), N-(3-sulfonic acid propyl group)-N methacrylamide propyl group-N (SPE), N '-dimethyl betaine (SPP) (Colloid Polym.Sci. (1990) 268) etc.
By the zwitterionic monomer polymerization that contains " N; N '-dimethyl " or and the multipolymer (as P (DMPS), P (AM/DMPS)) of neutral monomer, in the aqueous solution, solvability is bad, especially when high at DMPS content and molecular weight of copolymer is large, the time that dissolving need to be longer in water.Reason is that " N, the N '-dimethyl " on quaternary ammonium salt group is sterically hindered little, makes between negative ions group, easily to produce in molecule or intermolecular sat linkage in macromolecular chain, forms cross-linked structure, and solvability is poor.In view of in polymer molecule, when the alkyl connecting is when large, can hinder the rotation of molecular chain, have large sterically hinderedly, and alkyl belongs to hydrophobic group, mutually repels, therefore hindered the N of sulfonic group and quaternary ammonium with hydrophilic ionic group
+positive electronegativity and the combination that causes.Therefore we increase on quaternary ammonium salt group and connect the sterically hindered of alkyl, make negative ions group contact difficulty, weaken it and interact, and just can increase the water-soluble of polymer amine lactone.
Because zwitterionic monomer belongs to acid, alkali type inner salt, soluble in water, the method for suitable employing inverse emulsion polymerization and other neutral non-ionic monomer copolymerization, obtain the not aobvious electrical Amphiphatic high polymer amine lactone of entirety.And the high molecular polymer prepared of emulsion polymerization way have solid content high, dissolve fast, the relative molecular mass more uniform advantage that distributes.
In this patent, with connecting larger space steric hindrance alkyl methyl acrylyl oxy-ethyl-N on quaternary ammonium salt group, N '-diethyl-N-propanesulfonic acid amine salt (DEPS) and non-ionic acrylamide monomers copolymerization, prepare a kind of high molecular, soluble in water, there is the amine lactone type Amphiphatic high polymer (AM/DEPS) of anti-polyelectrolyte solution behavior, this polymkeric substance has significant salt tackify characteristic, can be applicable to multiple fields such as industrial novel material and additive, as oilfield exploitation, water treatment, water-absorbing material, medicine etc., especially can be used as the anti-salt oil-displacing agent that drilling fluid tackifier under high salinity and agent for improving oilfield recovery are used.
In sum, compared with prior art, the present invention has advantages of following outstanding:
1. the present invention adopts the preparation method of inverse emulsion polymerization, reaction process easily controls, simple to operate, the solid content of polymer emulsion is between 20～40%, and application molecular weight regulator can be controlled between 3～15dL/g the intrinsic viscosity of amine lactone type Amphiphatic high polymer.
2. amine lactone type amphoteric macromolecule polymer emulsion general performance in water with anti-polyelectrolyte solution behavior of the present invention goes out non-ionic copolymer characteristic, and has salt tackify characteristic.In fresh water and high-salinity brine, easily disperse, dissolve, apply very convenient.The finished product can directly be applied, and do not need long-time dispersion, have improved production efficiency.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Intrinsic viscosity is measured according to GB 12005.1-89 polyacrylamide For Intrinsic Viscosity Measurements method
Embodiment 1
Water: take acrylamide 28g, zwitterionic monomer DEPS (methylacryoyloxyethyl-N, N '-diethyl-N-propanesulfonic acid amine salt) 3g, be dissolved in 40g deionized water, add the aqueous solution 5g containing finite concentration complexing agent EDTA (disodium EDTA), logical nitrogen 20min.Oil phase: take HLB value and be 4.5 composite emulsifier 4.5g, mix with 30g white oil.Under high-speed stirring, lentamente water is added drop-wise in oil phase, fully stirs, form uniform W/O emulsion.Logical nitrogen deoxygenation 20min.Successively drip the aqueous solution 2mL of reductive agent and the aqueous solution 2mL of oxygenant to gradation in above-mentioned emulsion, be warming up to 30 DEG C, continue reaction 1～4 hour, obtain the amine lactone type amphiphilic polymers emulsion of oyster white homogeneous thickness.The amphiphilic polymers pulvis obtaining after ethanol precipitates, is dried, intrinsic viscosity is 14.9dL/g.
Embodiment 2
Water: take acrylamide 28g, zwitterionic monomer (DEPS) 6g, be dissolved in 40g deionized water, add the aqueous solution 5g containing finite concentration complexing agent EDTA, logical nitrogen 20min.Oil phase: take HLB value and be 4.5 composite emulsifier 4.5g, mix with 30g white oil.Under high-speed stirring, lentamente water is added drop-wise in oil phase, fully stirs, form uniform W/O emulsion.Logical nitrogen deoxygenation 20min.Successively drip the aqueous solution 2mL of reductive agent and the aqueous solution 2mL of oxygenant to gradation in above-mentioned emulsion, be warming up to 30 DEG C, continue reaction 1～4 hour, obtain the amine lactone type amphiphilic polymers emulsion of oyster white homogeneous thickness.The amine lactone type amphiphilic polymers pulvis obtaining after ethanol precipitates, is dried, intrinsic viscosity is 14.2dL/g.
Embodiment 3
Water: take acrylamide 28g, zwitterionic monomer (DEPS) 6g, be dissolved in 40g deionized water, add containing the aqueous solution 5g of finite concentration complexing agent EDTA and containing the aqueous solution 2g of finite concentration molecular weight regulator, logical nitrogen 20min.Oil phase: take HLB value and be 4.5 composite emulsifier 4.5g, mix with 30g white oil.Under high-speed stirring, lentamente water is added drop-wise in oil phase, fully stirs, form uniform W/O emulsion.Logical nitrogen deoxygenation 20min.Successively drip the aqueous solution 2mL of reductive agent and the aqueous solution 2mL of oxygenant to gradation in above-mentioned emulsion, be warming up to 30 DEG C, continue reaction 1～4 hour, obtain the amine lactone type amphiphilic polymers emulsion of oyster white homogeneous thickness.The amine lactone type amphiphilic polymers pulvis obtaining after ethanol precipitates, is dried, intrinsic viscosity is 9.6dL/g.
Embodiment 4
Water: take acrylamide 28g, zwitterionic monomer (DEPS) 6g, be dissolved in 40g deionized water, add containing the aqueous solution 5g of finite concentration complexing agent EDTA and containing the aqueous solution 4g of finite concentration molecular weight regulator, logical nitrogen 20min.Oil phase: take HLB value and be 4.5 composite emulsifier 4.5g, mix with 30g white oil.Under high-speed stirring, lentamente water is added drop-wise in oil phase, fully stirs, form uniform W/O emulsion.Logical nitrogen deoxygenation 20min.Successively drip the aqueous solution 2mL of reductive agent and the aqueous solution 2mL of oxygenant to gradation in above-mentioned emulsion, be warming up to 30 DEG C, continue reaction 1～4 hour, obtain the amine lactone type amphiphilic polymers emulsion of oyster white homogeneous thickness.The amine lactone type amphiphilic polymers pulvis obtaining after ethanol precipitates, is dried, intrinsic viscosity is 5.5dL/g.
Embodiment 5
Water: take N,N-DMAA 28g, zwitterionic monomer (DMPS) 8g, be dissolved in 45g deionized water, add the aqueous solution 5g of complexing agent EDTA, logical nitrogen 20min.Oil phase: take HLB value and be 4.3 emulsifying agent 4.5g, mix with 30g white oil.Under high-speed stirring, lentamente water is added drop-wise in oil phase, fully stirs, form uniform W/O emulsion.Logical nitrogen deoxygenation 20min.Successively drip in the aqueous solution 2mL of reductive agent and the aqueous solution 2mL water of oxygenant to gradation in above-mentioned emulsion, be warming up to 40 DEG C, continue reaction 1～4 hour, obtain the amphiphilic polymers emulsion of oyster white homogeneous thickness.The amine lactone type amphiphilic polymers pulvis obtaining after ethanol precipitates, is dried, intrinsic viscosity is 7.8dL/g.
Embodiment 6
Water: take acrylamide 20g, N,N-DMAA 10g, zwitterionic monomer (DMPS) 5g, be dissolved in 50g deionized water, add the aqueous solution 2g of complexing agent EDTA, logical nitrogen 20min.Oil phase: take HLB value and be 4.5 composite emulsifier 5g, mix with 40g white oil.Under high-speed stirring, lentamente water is added drop-wise in oil phase, fully stirs, form uniform W/O emulsion.Logical nitrogen deoxygenation 20min.Successively drip the aqueous solution 3mL of reductive agent and the aqueous solution 4mL of oxygenant to gradation in above-mentioned emulsion, be warming up to 40 DEG C, continue reaction 1～4 hour, obtain the amphiphilic polymers emulsion of oyster white homogeneous thickness.The amine lactone type amphiphilic polymers pulvis obtaining after ethanol precipitates, is dried, intrinsic viscosity is 11.3dL/g.
Claims (10)
1. an amine lactone type amphoteric macromolecule polymer emulsion, is characterized in that described emulsion comprises the polymkeric substance being obtained by sulphonic acid betaine type Amphiphatic high polymer monomer and the neutral monomer of following general formula:
The wherein integer of n=2～4;
Wherein R is selected from one of lower array structure:
CH
2=CH-COOCH
2CH
2-，CH
2=CH-CONHCH
2CH
2-
2. amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 1, is characterized in that:
Described amine lactone type amphoteric macromolecule polymer emulsion is to prepare as raw material adopts inverse emulsion polymerization taking the component of following weight percent, wherein,
Non-ionic acrylamide monomers 10～35%;
Sulphonic acid betaine type zwitterionic monomer 3～20%;
Oil phase 10～30%;
Initiator 0.1～0.8%;
Emulsifying agent 3～10%;
Molecular weight regulator 0.01～0.5%;
Water surplus.
3. amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 2, is characterized in that:
Described non-ionic acrylamide monomers is selected from acrylamide, N hydroxymethyl acrylamide, N,N-DMAA, N-ethyl acrylamide, N, the combination of one or more in N-diethyl acrylamide, N-propyl group acrylamide;
Described oil phase is selected from alkane, diesel oil, aviation kerosene, white oil;
Described initiator is made up of Oxidizing and Reducing Agents, and oxygenant is wherein selected from the one in Potassium Persulphate, ammonium persulphate, hydrogen peroxide, and reductive agent is selected from the one in sodium bisulfite, Tetramethyl Ethylene Diamine;
Described molecular weight regulator is the compound that contains sulfydryl;
Described emulsifying agent is non-ionic type compound emulsifying agent.
4. amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 3, is characterized in that:
Described oil phase is 5～26# white oil;
Described non-ionic type compound emulsifying agent carries out composite making by spans tensio-active agent and Tweens tensio-active agent or polyethenoxy ether class tensio-active agent;
The HLB value of described non-ionic type compound emulsifying agent is 4～7.
5. amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 4, is characterized in that:
Described spans tensio-active agent is selected from least one in Span-85, Span-80, Span-60; Described Tweens tensio-active agent is selected from least one in Tween-80, Tween-60; Described polyethenoxy ether class tensio-active agent is OP-10;
The HLB value of described non-ionic type compound emulsifying agent is 4.5～5.5.
6. the preparation method of the amine lactone type amphoteric macromolecule polymer emulsion as described in one of claim 1～5, is characterized in that:
Described amine lactone type amphoteric macromolecule polymer emulsion adopts the preparation method of inverse emulsion polymerization.
7. the preparation method of amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 6, is characterized in that the method comprises the steps:
(1) prepare water: by water miscible zwitterionic monomer and acrylamide monomers, and molecular weight regulator is dissolved in deionized water, logical nitrogen deoxygenation, adds complexing agent;
(2) prepare oil phase: composite emulsifying agent is dissolved in to white oil, fully stirs, emulsifying agent is fully dissolved, form uniform oil-phase solution;
(3) emulsification: under high-speed stirring, water is slowly splashed in oil phase, logical nitrogen deoxygenation 20～30 minutes, forms uniform tiny emulsion;
(4) polyreaction: drip the aqueous solution of reductive agent and the aqueous solution of oxygenant in the good water-in-oil emulsion of above-mentioned emulsification, keeping temperature is 20～60 DEG C, continues reaction 1～4 hour, obtains the amine lactone type emulsion polymerization of oyster white homogeneous thickness.
8. the preparation method of amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 7, is characterized in that:
Described complexing agent is disodium edta.
9. the conduct in oilfield exploitation, water treatment, water-absorbing material, medicine of the amine lactone type amphoteric macromolecule polymer emulsion as described in one of claim 1～5 has the purposes of salt tackify effect.
10. the purposes of the anti-salt oil-displacing agent that amine lactone type amphoteric macromolecule polymer emulsion as claimed in claim 9 drilling fluid tackifier and agent for improving oilfield recovery under high salinity used.
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